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采用高效液相色谱-串联质谱仪(HPLC-MS/MS)建立了蔬菜中麦草畏的残留分析方法,其中蔬菜基质包括白菜、黄瓜、番茄、豇豆、萝卜、芹菜和葱。样品经V(乙腈):V(甲酸):V(水)=49.5:0.2:0.3的混合溶剂提取,并用氯化钠盐析,旋转蒸发浓缩后直接用HPLC-MS/MS测定。采用C18色谱柱,以5 mmol/L的甲酸铵-甲醇为流动相,梯度法洗脱,以电喷雾负离子化模式在多反应监测模式下测定。结果表明,麦草畏在0.005～0.5 mg/L范围内线性关系良好,相关系数(r)为0.999 7。对空白蔬菜样品进行的3个水平(0.01、0.05、0.1mg/kg)的添加回收实验结果表明,麦草畏的平均回收率和相对标准偏差(RSD)分别为80%～120%和0.58%～18.23%,方法检出限为2.0μg/kg。该方法快速、灵敏,适用于蔬菜中麦草畏的残留分析。
Residues of dicamba in vegetables were established by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). The vegetable matrix included cabbage, cucumber, tomato, cowpea, radish, celery and onion. The sample was extracted with a mixed solvent of V (acetonitrile): V (formic acid): V (water) = 49.5: 0.2: 0.3 and salted out with sodium chloride and concentrated by rotary evaporation and directly determined by HPLC-MS / MS. C18 column with 5 mmol / L ammonium formate-methanol as the mobile phase, gradient elution, electrospray ionization mode in the multi-reaction monitoring mode determination. The results showed that dicamba had a good linear relationship in the range of 0.005-0.5 mg / L with a correlation coefficient (r) of 0.999 7. The results of the recovery experiments of blank vegetable samples at three levels (0.01, 0.05 and 0.1 mg / kg) showed that the average recoveries and relative standard deviations (RSDs) of dicamba were 80% -120% and 0.58% 18.23%, the detection limit of method is 2.0μg / kg. The method is fast and sensitive and is suitable for the analysis of dicamba residue in vegetables.